# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 1145/180 data_S487/1 #------------------------------------------------------------------------------ _audit_creation_date '1999-04-22' _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; #------------------------------------------------------------------------------ _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The non-hydrogen atoms were refined anisotropically. The hydrogen atoms were included in the structure factor calculation in idealised positions, and were assigned isotropic thermal parameters which were 20% greater than the equivalent B value of the atom to which they were bonded. ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Altomare, A., Cascarano, M., Giacovazzo, C., Guagliardi, A. (1993). J. Appl. Cryst., 26, 343. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1995)' _computing_structure_solution ; SIR92 (Altomare, et. al. 1993) ; _computing_structure_refinement 'teXsan (MSC, 1995)' _computing_publication_material 'teXsan (MSC, 1995)' #------------------------------------------------------------------------------ _cell_length_a 27.653(7) _cell_length_b 8.130(2) _cell_length_c 9.857(4) _cell_angle_alpha 90 _cell_angle_beta 95.74(4) _cell_angle_gamma 90 _cell_volume 2204(2) _cell_formula_units_Z 4 _cell_measurement_temperature 290.2 _cell_measurement_reflns_used 12 _cell_measurement_theta_min 7.8 _cell_measurement_theta_max 11.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colourlessprismatic' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 368.56 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H40 O4 ' _chemical_formula_moiety 'C22 H40 O4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 816.00 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type ; \y scans (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.951 _exptl_special_details ; The scan width was (1.05+0.30tan\q)\% with an \w scan speed of 8\% per minute (up to 4 scans to achieve I/\s(I) > 10). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 290.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.20 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 4486 _reflns_number_total 4226 _reflns_number_observed 1767 _reflns_observed_criterion >3.00\s(I) _diffrn_reflns_av_R_equivalents 0.03035 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00330 _diffrn_orient_matrix_UB_12 -0.09147 _diffrn_orient_matrix_UB_13 0.06627 _diffrn_orient_matrix_UB_21 -0.03619 _diffrn_orient_matrix_UB_22 0.00669 _diffrn_orient_matrix_UB_23 -0.01779 _diffrn_orient_matrix_UB_31 0.00072 _diffrn_orient_matrix_UB_32 -0.08197 _diffrn_orient_matrix_UB_33 -0.07542 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 88 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 160 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 16 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom O1 0.06259(8) 0.4304(3) 0.0689(2) 0.0562(9) 1.000 . Uani d ? O2 0.01443(9) 0.3525(4) 0.2267(3) 0.075(1) 1.000 . Uani d ? O3 0.44520(8) 0.3626(4) 0.5691(3) 0.0601(9) 1.000 . Uani d ? O4 0.4513(1) 0.4541(4) 0.7828(3) 0.088(1) 1.000 . Uani d ? C1 0.0400(1) 0.3181(5) 0.1404(4) 0.053(1) 1.000 . Uani d ? C2 0.0519(1) 0.1472(5) 0.0974(4) 0.060(1) 1.000 . Uani d ? C3 0.1063(1) 0.1152(5) 0.0987(4) 0.055(1) 1.000 . Uani d ? C4 0.1346(1) 0.1358(5) 0.2371(3) 0.053(1) 1.000 . Uani d ? C5 0.1888(1) 0.1249(5) 0.2318(3) 0.055(1) 1.000 . Uani d ? C6 0.2187(1) 0.1364(5) 0.3686(3) 0.054(1) 1.000 . Uani d ? C7 0.2727(1) 0.1405(5) 0.3593(3) 0.054(1) 1.000 . Uani d ? C8 0.3035(1) 0.1416(5) 0.4951(3) 0.056(1) 1.000 . Uani d ? C9 0.3572(1) 0.1598(5) 0.4851(3) 0.051(1) 1.000 . Uani d ? C10 0.3878(1) 0.1521(5) 0.6211(4) 0.058(1) 1.000 . Uani d ? C11 0.4407(1) 0.1951(5) 0.6137(4) 0.066(2) 1.000 . Uani d ? C12 0.4486(1) 0.4822(6) 0.6636(4) 0.056(1) 1.000 . Uani d ? C13 0.4489(1) 0.6469(5) 0.6005(4) 0.060(1) 1.000 . Uani d ? C14 0.4111(1) 0.6708(5) 0.4792(4) 0.060(1) 1.000 . Uani d ? C15 0.3593(1) 0.6552(5) 0.5139(4) 0.055(1) 1.000 . Uani d ? C16 0.3221(1) 0.6575(5) 0.3900(4) 0.056(1) 1.000 . Uani d ? C17 0.2699(1) 0.6487(5) 0.4211(4) 0.056(1) 1.000 . Uani d ? C18 0.2339(1) 0.6418(5) 0.2958(4) 0.056(1) 1.000 . Uani d ? C19 0.1813(1) 0.6463(5) 0.3235(4) 0.055(1) 1.000 . Uani d ? C20 0.1456(1) 0.6282(5) 0.1983(4) 0.053(1) 1.000 . Uani d ? C21 0.0930(1) 0.6433(5) 0.2272(4) 0.055(1) 1.000 . Uani d ? C22 0.0570(1) 0.6008(5) 0.1084(4) 0.061(1) 1.000 . Uani d ? H2A 0.0390 0.0715 0.1577 0.073 1.000 . Uiso c ? H2B 0.0371 0.1290 0.0072 0.073 1.000 . Uiso c ? H3A 0.1108 0.0056 0.0691 0.067 1.000 . Uiso c ? H3B 0.1191 0.1898 0.0374 0.067 1.000 . Uiso c ? H4A 0.1272 0.2405 0.2723 0.064 1.000 . Uiso c ? H4B 0.1250 0.0521 0.2958 0.064 1.000 . Uiso c ? H5A 0.1958 0.0225 0.1919 0.066 1.000 . Uiso c ? H5B 0.1984 0.2120 0.1764 0.066 1.000 . Uiso c ? H6A 0.2097 0.2341 0.4125 0.066 1.000 . Uiso c ? H6B 0.2114 0.0436 0.4215 0.066 1.000 . Uiso c ? H7A 0.2812 0.0460 0.3103 0.065 1.000 . Uiso c ? H7B 0.2800 0.2368 0.3111 0.065 1.000 . Uiso c ? H8A 0.2932 0.2306 0.5474 0.068 1.000 . Uiso c ? H8B 0.2983 0.0409 0.5403 0.068 1.000 . Uiso c ? H9A 0.3672 0.0741 0.4290 0.062 1.000 . Uiso c ? H9B 0.3625 0.2632 0.4445 0.062 1.000 . Uiso c ? H10A 0.3747 0.2267 0.6816 0.070 1.000 . Uiso c ? H10B 0.3861 0.0432 0.6555 0.070 1.000 . Uiso c ? H11A 0.4541 0.1230 0.5517 0.080 1.000 . Uiso c ? H11B 0.4577 0.1820 0.7020 0.080 1.000 . Uiso c ? H13A 0.4432 0.7264 0.6682 0.073 1.000 . Uiso c ? H13B 0.4801 0.6650 0.5710 0.073 1.000 . Uiso c ? H14A 0.4151 0.7776 0.4432 0.073 1.000 . Uiso c ? H14B 0.4163 0.5905 0.4129 0.073 1.000 . Uiso c ? H15A 0.3562 0.5543 0.5611 0.067 1.000 . Uiso c ? H15B 0.3526 0.7441 0.5719 0.067 1.000 . Uiso c ? H16A 0.3263 0.7563 0.3417 0.068 1.000 . Uiso c ? H16B 0.3282 0.5658 0.3348 0.068 1.000 . Uiso c ? H17A 0.2659 0.5528 0.4738 0.069 1.000 . Uiso c ? H17B 0.2631 0.7434 0.4723 0.069 1.000 . Uiso c ? H18A 0.2398 0.7333 0.2400 0.068 1.000 . Uiso c ? H18B 0.2393 0.5428 0.2488 0.068 1.000 . Uiso c ? H19A 0.1759 0.5591 0.3842 0.067 1.000 . Uiso c ? H19B 0.1753 0.7485 0.3651 0.067 1.000 . Uiso c ? H20A 0.1523 0.7111 0.1349 0.065 1.000 . Uiso c ? H20B 0.1501 0.5229 0.1596 0.065 1.000 . Uiso c ? H21A 0.0878 0.5719 0.3002 0.068 1.000 . Uiso c ? H21B 0.0874 0.7538 0.2527 0.068 1.000 . Uiso c ? H22A 0.0622 0.6702 0.0334 0.074 1.000 . Uiso c ? H22B 0.0250 0.6173 0.1331 0.074 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.051(2) 0.061(2) 0.056(2) -0.005(1) 0.001(1) -0.001(2) O2 0.065(2) 0.075(2) 0.089(2) 0.004(2) 0.031(2) 0.004(2) O3 0.055(2) 0.066(2) 0.059(2) -0.007(2) 0.002(1) -0.003(2) O4 0.114(2) 0.100(3) 0.049(2) -0.011(2) -0.004(2) 0.003(2) C1 0.037(2) 0.061(3) 0.059(3) -0.004(2) -0.009(2) 0.002(2) C2 0.051(3) 0.063(3) 0.064(3) -0.005(2) -0.008(2) -0.007(2) C3 0.055(2) 0.053(3) 0.055(3) 0.004(2) -0.001(2) -0.008(2) C4 0.051(2) 0.056(3) 0.050(2) 0.003(2) 0.001(2) 0.001(2) C5 0.053(2) 0.056(3) 0.053(2) 0.009(2) 0.000(2) -0.001(2) C6 0.049(2) 0.061(3) 0.052(2) 0.002(2) 0.003(2) 0.001(2) C7 0.057(2) 0.053(3) 0.050(2) -0.001(2) 0.002(2) 0.000(2) C8 0.051(2) 0.065(3) 0.050(2) -0.004(2) 0.000(2) 0.002(2) C9 0.049(2) 0.055(3) 0.048(2) -0.003(2) 0.001(2) 0.001(2) C10 0.057(2) 0.064(3) 0.051(2) -0.005(2) -0.005(2) 0.010(2) C11 0.060(3) 0.061(3) 0.075(3) 0.005(2) -0.010(2) 0.001(2) C12 0.039(2) 0.075(3) 0.053(3) -0.009(2) -0.003(2) -0.002(3) C13 0.046(2) 0.068(3) 0.065(3) -0.013(2) 0.005(2) -0.003(3) C14 0.056(2) 0.063(3) 0.061(3) -0.003(2) 0.008(2) 0.006(2) C15 0.050(2) 0.059(3) 0.057(2) -0.001(2) 0.008(2) -0.004(2) C16 0.052(2) 0.061(3) 0.054(2) -0.001(2) 0.002(2) -0.001(2) C17 0.049(2) 0.061(3) 0.058(3) -0.001(2) 0.001(2) 0.001(2) C18 0.049(2) 0.059(3) 0.058(2) 0.002(2) 0.004(2) 0.001(2) C19 0.051(2) 0.056(3) 0.058(2) -0.004(2) 0.002(2) 0.000(2) C20 0.050(2) 0.053(3) 0.056(2) -0.001(2) 0.001(2) 0.001(2) C21 0.050(2) 0.052(3) 0.064(3) 0.003(2) 0.001(2) -0.004(2) C22 0.061(3) 0.052(3) 0.068(3) 0.005(2) -0.002(2) 0.008(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00000|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1767 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0497 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0354 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.775 _refine_ls_shift/esd_max 0.0003 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.13 _refine_diff_density_max 0.16 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.345(5) . . yes O1 C22 1.451(5) . . yes O2 C1 1.193(5) . . yes O3 C11 1.441(5) . . yes O3 C12 1.342(5) . . yes O4 C12 1.192(5) . . yes C1 C2 1.499(6) . . yes C2 C3 1.526(5) . . yes C2 H2A 0.95 . . no C2 H2B 0.95 . . no C3 C4 1.512(5) . . yes C3 H3A 0.95 . . no C3 H3B 0.95 . . no C4 C5 1.508(5) . . yes C4 H4A 0.95 . . no C4 H4B 0.95 . . no C5 C6 1.511(4) . . yes C5 H5A 0.95 . . no C5 H5B 0.95 . . no C6 C7 1.507(5) . . yes C6 H6A 0.95 . . no C6 H6B 0.95 . . no C7 C8 1.512(4) . . yes C7 H7A 0.95 . . no C7 H7B 0.95 . . no C8 C9 1.505(5) . . yes C8 H8A 0.95 . . no C8 H8B 0.95 . . no C9 C10 1.514(5) . . yes C9 H9A 0.95 . . no C9 H9B 0.95 . . no C10 C11 1.511(5) . . yes C10 H10A 0.95 . . no C10 H10B 0.95 . . no C11 H11A 0.95 . . no C11 H11B 0.95 . . no C12 C13 1.477(6) . . yes C13 C14 1.520(5) . . yes C13 H13A 0.95 . . no C13 H13B 0.95 . . no C14 C15 1.510(5) . . yes C14 H14A 0.95 . . no C14 H14B 0.95 . . no C15 C16 1.516(5) . . yes C15 H15A 0.95 . . no C15 H15B 0.95 . . no C16 C17 1.507(5) . . yes C16 H16A 0.95 . . no C16 H16B 0.95 . . no C17 C18 1.508(5) . . yes C17 H17A 0.95 . . no C17 H17B 0.95 . . no C18 C19 1.509(5) . . yes C18 H18A 0.95 . . no C18 H18B 0.95 . . no C19 C20 1.508(5) . . yes C19 H19A 0.95 . . no C19 H19B 0.95 . . no C20 C21 1.517(5) . . yes C20 H20A 0.95 . . no C20 H20B 0.95 . . no C21 C22 1.499(5) . . yes C21 H21A 0.95 . . no C21 H21B 0.95 . . no C22 H22A 0.95 . . no C22 H22B 0.95 . . no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C22 116.1(3) . . . yes C11 O3 C12 118.4(3) . . . yes O1 C1 O2 123.6(4) . . . yes O1 C1 C2 110.8(3) . . . yes O2 C1 C2 125.6(4) . . . yes C1 C2 C3 113.6(3) . . . yes C1 C2 H2A 108.5 . . . no C1 C2 H2B 108.8 . . . no C3 C2 H2A 108.5 . . . no C3 C2 H2B 108.2 . . . no H2A C2 H2B 109.3 . . . no C2 C3 C4 114.2(3) . . . yes C2 C3 H3A 108.4 . . . no C2 C3 H3B 108.3 . . . no C4 C3 H3A 108.1 . . . no C4 C3 H3B 108.2 . . . no H3A C3 H3B 109.7 . . . no C3 C4 C5 112.9(3) . . . yes C3 C4 H4A 108.5 . . . no C3 C4 H4B 108.7 . . . no C5 C4 H4A 108.5 . . . no C5 C4 H4B 108.6 . . . no H4A C4 H4B 109.6 . . . no C4 C5 C6 114.9(3) . . . yes C4 C5 H5A 108.0 . . . no C4 C5 H5B 108.1 . . . no C6 C5 H5A 108.0 . . . no C6 C5 H5B 108.1 . . . no H5A C5 H5B 109.7 . . . no C5 C6 C7 113.8(3) . . . yes C5 C6 H6A 108.3 . . . no C5 C6 H6B 108.4 . . . no C7 C6 H6A 108.3 . . . no C7 C6 H6B 108.4 . . . no H6A C6 H6B 109.6 . . . no C6 C7 C8 114.8(3) . . . yes C6 C7 H7A 108.0 . . . no C6 C7 H7B 108.1 . . . no C8 C7 H7A 108.1 . . . no C8 C7 H7B 108.1 . . . no H7A C7 H7B 109.7 . . . no C7 C8 C9 114.4(3) . . . yes C7 C8 H8A 108.2 . . . no C7 C8 H8B 108.2 . . . no C9 C8 H8A 108.2 . . . no C9 C8 H8B 108.1 . . . no H8A C8 H8B 109.6 . . . no C8 C9 C10 114.0(3) . . . yes C8 C9 H9A 108.3 . . . no C8 C9 H9B 108.2 . . . no C10 C9 H9A 108.4 . . . no C10 C9 H9B 108.2 . . . no H9A C9 H9B 109.7 . . . no C9 C10 C11 114.0(3) . . . yes C9 C10 H10A 108.3 . . . no C9 C10 H10B 108.1 . . . no C11 C10 H10A 108.4 . . . no C11 C10 H10B 108.4 . . . no H10A C10 H10B 109.6 . . . no O3 C11 C10 110.3(3) . . . yes O3 C11 H11A 109.7 . . . no O3 C11 H11B 109.5 . . . no C10 C11 H11A 109.2 . . . no C10 C11 H11B 108.8 . . . no H11A C11 H11B 109.3 . . . no O3 C12 O4 122.6(4) . . . yes O3 C12 C13 111.5(3) . . . yes O4 C12 C13 125.9(4) . . . yes C12 C13 C14 114.5(3) . . . yes C12 C13 H13A 108.1 . . . no C12 C13 H13B 108.3 . . . no C14 C13 H13A 108.3 . . . no C14 C13 H13B 108.3 . . . no H13A C13 H13B 109.3 . . . no C13 C14 C15 113.9(3) . . . yes C13 C14 H14A 108.3 . . . no C13 C14 H14B 108.3 . . . no C15 C14 H14A 108.1 . . . no C15 C14 H14B 108.2 . . . no H14A C14 H14B 110.0 . . . no C14 C15 C16 113.6(3) . . . yes C14 C15 H15A 108.5 . . . no C14 C15 H15B 108.6 . . . no C16 C15 H15A 108.5 . . . no C16 C15 H15B 108.5 . . . no H15A C15 H15B 109.1 . . . no C15 C16 C17 115.0(3) . . . yes C15 C16 H16A 108.0 . . . no C15 C16 H16B 107.9 . . . no C17 C16 H16A 108.0 . . . no C17 C16 H16B 107.9 . . . no H16A C16 H16B 110.0 . . . no C16 C17 C18 113.7(3) . . . yes C16 C17 H17A 108.4 . . . no C16 C17 H17B 108.4 . . . no C18 C17 H17A 108.3 . . . no C18 C17 H17B 108.4 . . . no H17A C17 H17B 109.5 . . . no C17 C18 C19 114.9(3) . . . yes C17 C18 H18A 108.0 . . . no C17 C18 H18B 108.0 . . . no C19 C18 H18A 108.0 . . . no C19 C18 H18B 108.0 . . . no H18A C18 H18B 109.7 . . . no C18 C19 C20 114.4(3) . . . yes C18 C19 H19A 108.2 . . . no C18 C19 H19B 108.2 . . . no C20 C19 H19A 108.2 . . . no C20 C19 H19B 108.2 . . . no H19A C19 H19B 109.7 . . . no C19 C20 C21 113.6(3) . . . yes C19 C20 H20A 108.4 . . . no C19 C20 H20B 108.4 . . . no C21 C20 H20A 108.6 . . . no C21 C20 H20B 108.4 . . . no H20A C20 H20B 109.5 . . . no C20 C21 C22 114.1(3) . . . yes C20 C21 H21A 108.2 . . . no C20 C21 H21B 108.0 . . . no C22 C21 H21A 108.3 . . . no C22 C21 H21B 108.3 . . . no H21A C21 H21B 109.9 . . . no O1 C22 C21 110.5(3) . . . yes O1 C22 H22A 109.3 . . . no O1 C22 H22B 109.3 . . . no C21 C22 H22A 109.3 . . . no C21 C22 H22B 109.2 . . . no H22A C22 H22B 109.3 . . . no #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 . . . . 51.7(4) no O1 C22 C21 C20 . . . . 62.1(4) no O2 C1 O1 C22 . . . . 4.0(5) no O2 C1 C2 C3 . . . . -127.7(4) no O3 C11 C10 C9 . . . . 62.7(4) no O3 C12 C13 C14 . . . . 44.9(4) no O4 C12 O3 C11 . . . . 5.2(5) no O4 C12 C13 C14 . . . . -135.7(4) no C1 O1 C22 C21 . . . . 83.2(4) no C1 C2 C3 C4 . . . . 60.4(4) no C2 C1 O1 C22 . . . . -175.4(3) no C2 C3 C4 C5 . . . . -172.6(3) no C3 C4 C5 C6 . . . . -177.1(3) no C4 C5 C6 C7 . . . . -174.8(3) no C5 C6 C7 C8 . . . . -176.5(3) no C6 C7 C8 C9 . . . . -175.2(3) no C7 C8 C9 C10 . . . . -177.0(3) no C8 C9 C10 C11 . . . . -171.5(3) no C10 C11 O3 C12 . . . . 87.9(4) no C11 O3 C12 C13 . . . . -175.4(3) no C12 C13 C14 C15 . . . . 62.4(4) no C13 C14 C15 C16 . . . . -172.6(3) no C14 C15 C16 C17 . . . . -177.8(3) no C15 C16 C17 C18 . . . . -176.8(3) no C16 C17 C18 C19 . . . . -175.4(3) no C17 C18 C19 C20 . . . . -176.2(3) no C18 C19 C20 C21 . . . . -176.5(3) no C19 C20 C21 C22 . . . . -171.3(3) no #------------------------------------------------------------------------------